HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triphenylphosphine → HCID 18348639, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | 4-Cyanophenol | HCID 13019 | — |
| Reactant | ethyl N-ethoxycarbonyliminocarbamate | HCID 220568 | — |
| Reactant | 7-(2-Hydroxyethyl)-2,3-dimethoxy-4,5,6,7,8,9-hexahydro-1H-benzo[a]cycloheptene-1,4-dione | HCID 18348573 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 18348639 | HCID 18348639 | 84.2% |
Reaction Steps
To a solution of 7-(2-hydroxyethyl)-2,3-dimethoxy-4,5,6,7,8,9-hexahydro-1H-benzo[a]cycloheptene-1,4-dione (103 mg), p-cyanophenol (127 mg), triphenylphosphine (126 mg) in THF (2 ml) was added a solution of diethyl azodicarboxylate (90 mg) in THF (1 ml) at room temperature. The reaction mixture was stirred at room temperature for 2 hr and then concentrated in vacuo. The residue was purified by alumina column chromatography (ethyl acetate:hexane=1:4) and then with recrystallization from ethyl acetate-hexane to obtain the entitled compound (118 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06326369B1 |
| Source dataset | uspto-grants-2001_12 |
| ORD ID | ord-bc3f180d015b4a249c4d7dba51c8d9fa |
| Source note | uspto-grants-2001_12 |